CN110885683A - Bi2MoO6Quantum dot and preparation method and application thereof - Google Patents
Bi2MoO6Quantum dot and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002096 quantum dot Substances 0.000 claims abstract description 85
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 229910002900 Bi2MoO6 Inorganic materials 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 35
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 21
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims abstract description 17
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 17
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 17
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000011941 photocatalyst Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 229910001220 stainless steel Inorganic materials 0.000 abstract 1
- 239000010935 stainless steel Substances 0.000 abstract 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 66
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 42
- 235000019445 benzyl alcohol Nutrition 0.000 description 22
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 21
- 238000001914 filtration Methods 0.000 description 19
- 230000003287 optical effect Effects 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 238000007789 sealing Methods 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 238000001514 detection method Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 229910052724 xenon Inorganic materials 0.000 description 10
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 10
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/7457—Vanadates; Chromates; Molybdates; Tungstates
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- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a Bi2MoO6Quantum dots, and a preparation method and application thereof, belonging to the quantum dot technologyThe field of the technology. The method comprises the following steps: dispersing bismuth nitrate pentahydrate and sodium oleate in water, and fully stirring; then adding sodium molybdate, continuously stirring and uniformly mixing, transferring the mixture into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction, after the reaction is finished, centrifugally collecting precipitate, respectively centrifugally washing the precipitate with water and ethanol for three times, and drying the precipitate to obtain Bi2MoO6Quantum dots, used as photocatalysts. Bi prepared by the invention2MoO6The quantum dot has small size and high catalytic performance, and the preparation method has the advantages of simplicity, easiness in industrial production and the like.
Description
Technical Field
The invention belongs to the technical field of quantum dots; in particular to Bi2MoO6Quantum dots and methods of making the same.
Background
With the rapid development of industrial activities, environmental pollution has become a global challenge. In order to solve these problems, development of a technique for remedying environmental pollution, which is reproducible and environmentally friendly, is urgently required. Among the many proposed technologies, semiconductor photocatalytic technology has received wide attention worldwide due to its ability to directly utilize solar energy to degrade harmful pollutants and produce hydrogen. Titanium dioxide (TiO)2) Is one of the most widely used photocatalyst systems. However, due to TiO2Has a large band gap (3.0-3.2eV), absorbs only the ultraviolet region (about 5%), and has little response to visible light in the solar spectrum (about 45%). Therefore, the development of high-efficiency photocatalysts utilizing visible light is a research hotspot in the field of photocatalyst research at present.
In recent years, bismuth-based semiconductors have received much attention as typical visible light-responsive photocatalysts. Bi2MoO6Is a typical Aurivillius structure semiconductor and has good chemical stability, proper band gap and optical activity. Bi2MoO6Sharing of [ Bi ] by oxygen2O2]2+Radical and perovskite type [ MO4]2-And (3) layer composition. The special layered structure has an internal electric field, which can ensure the rapid separation of photo-generated charges. Thus, Bi2MoO6Is a promising semiconductor material and can improve the photocatalytic utilization of solar energy. In general, the photocatalytic performance of a photocatalyst depends largely on its morphology and structure. Therefore, the preparation of the nano material with an ideal structure has important significance for obtaining good photocatalytic performance. At present, Bi with different shapes including hollow spherical structures, graded mesoporous clusters, micro-flowers and the like2MoO6Semiconductors have been successfully prepared, and these articles indicate that increasing the specific surface area of semiconductors is effective in enhancing the interaction between the photocatalyst and the substrate, thereby improving photocatalytic performance.
The quantum dot has ultrahigh specific surface area, and the preparation of the semiconductor quantum dot is one of approaches for improving the photocatalytic performance of the semiconductor, but because the preparation of the quantum dot is difficult, Bi is difficult at present2MoO6Quantum dots have been reported rarely.
Disclosure of Invention
The invention aims to solve the problem of Bi2MoO6The quantum dots are difficult to prepare, the process is complex and the like. The invention provides a hydrothermal preparation method of Bi2MoO6The method for preparing the quantum dots has the advantages of simple operation, low production cost, easy large-scale industrial production and the like.
One kind of Bi in the present invention2MoO6The quantum dots are prepared by taking pentahydrate bismuth nitrate and sodium molybdate as raw materials and sodium oleate as a surfactant by a hydrothermal method; the method specifically comprises the following steps:
dispersing pentahydrate bismuth nitrate and sodium oleate in water, and stirring for 0.5-1 h. Then adding sodium molybdate, and continuing stirring for 1-2 h;
step two, carrying out hydrothermal reaction, after the reaction is finished, centrifugally separating and collecting precipitates, respectively centrifugally washing the precipitates for at least 3 times by using water and absolute ethyl alcohol, and drying the precipitates to obtain Bi2MoO6And (4) quantum dots.
Further limiting, in the first step, the molar ratio of the bismuth nitrate pentahydrate to the sodium molybdate is 2: 1.
Further limiting, the molar ratio of the bismuth nitrate pentahydrate to the sodium oleate in the step one is 1 (2-6).
Further limiting, the ratio of the mole of the bismuth nitrate pentahydrate to the volume of the water in the first step is 1mmol (20-80) mL.
Further, the stirring is carried out at a speed of 500r/m to 1000r/m in the first step.
Further limiting, in the second step, carrying out hydrothermal reaction for 10-24 h at 160-200 ℃.
Further limiting, the second step is dried for 12 to 24 hours at the temperature of between 60 and 80 ℃.
The invention provides a simple hydrothermal method for preparing Bi2MoO6The method of the quantum dots has the advantages of simple preparation process, easy industrial expanded production and the like.
The invention avoids quantum dot polymerization.
Bi prepared by the method of the invention2MoO6The quantum dots are small in size, only about 5nm, large in specific surface area and excellent in photocatalytic oxidation performance, can be directly used as a photocatalyst, and can oxidize benzyl alcohol into benzaldehyde at normal temperature and normal pressure, and the photocatalytic oxidation technology is expected to replace the traditional high-temperature high-pressure oxidation technology, so that the novel green oxidation technology is formed, and the problems of environmental pollution and energy shortage are solved.
Drawings
FIG. 1 shows Bi2MoO6An X-ray powder diffraction test chart of the quantum dots;
FIG. 2 shows Bi2MoO6A transmission electron micrograph of the quantum dots;
FIG. 3 shows Bi2MoO6And (5) testing the performance of the benzyl alcohol oxidized by the quantum dot photocatalysis.
Detailed Description
Example 1, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 0.5mmol of pentahydrate bismuth nitrate and 2mmol of sodium oleate into 20mL of water, stirring at the speed of 500r/m for 1h, then adding 0.25mmol of sodium molybdate, stirring at the speed of 500r/m for 1h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 180 ℃ for 12h, centrifuging to collect precipitate, then carrying out centrifugal washing with water for three times, carrying out centrifugal washing with absolute ethyl alcohol for three times, and drying at 60 ℃ for 12h to obtain Bi2MoO6And (4) quantum dots.
FIG. 1 shows Bi2MoO6X-ray powder diffraction test pattern of quantum dots. It can be seen from the figure that the prepared solid powder X-ray derived peaks compare with the standard card JCPDS: 84-0787 are completely identical, indicating that the solid powder obtained is pure Bi2MoO6The crystal is a mixture of a crystal and a metal,FIG. 2 is Bi2MoO6The transmission electron microscope picture of the quantum dot can show that the Bi is obtained2MoO6The quantum dot size is about 5 nm.
Bi prepared in this example was taken2MoO6Dispersing 15mg of quantum dots in 1.5mL of water, adding 10.4 microliter of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at 1000r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after 4h of irradiation, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 4 hours under visible light, the conversion rate of the benzyl alcohol to the benzaldehyde is 50%, and the selectivity is more than 99% (fig. 3).
Example 2, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 1mmol of pentahydrate bismuth nitrate and 2mmol of sodium oleate into 20mL of water, stirring at the speed of 800r/m for 0.5h, then adding 0.5mmol of sodium molybdate, stirring at the speed of 800r/m for 1h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 200 ℃ for 10h, centrifuging, collecting precipitate, respectively carrying out centrifugal washing with water and absolute ethyl alcohol for three times, and drying at 60 ℃ for 24h to obtain Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 15mg of quantum dots in 1.5mL of water, adding 10.4 microliter of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at 1000r/m for 40m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after 4h of irradiation, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 4 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 45 percent, and the selectivity is more than 99 percent。
Example 3, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 0.5mmol of pentahydrate bismuth nitrate and 1mmol of sodium oleate into 40mL of water, stirring at the speed of 600r/m for 1h, then adding 0.25mmol of sodium molybdate, stirring at the speed of 600r/m for 2h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 160 ℃ for 24h, centrifuging, collecting precipitate, respectively carrying out centrifugal washing with water and absolute ethyl alcohol for three times, drying at 60 ℃ for 15h, and obtaining Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 17mg of quantum dots in 1.5mL of water, adding 10.4 microliters of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at the speed of 800r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after the light is irradiated for 5 hours, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 5 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 55%, and the selectivity is more than 99%.
Example 4, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 0.5mmol of pentahydrate bismuth nitrate and 3mmol of sodium oleate into 30mL of water, stirring at the speed of 700r/m for 0.5h, then adding 0.25mmol of sodium molybdate, stirring at the speed of 700r/m for 1.5h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 180 ℃ for 20h, centrifuging, collecting precipitate, centrifuging and washing with water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ for 16h to obtain Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 15mg of quantum dots in 1.5mL of water, adding 10.4 microliter of benzyl alcohol, introducing oxygen to discharge air in the reaction flask, sealing, and sealing by 10Stirring at a speed of 00r/m for 60m, starting a 500W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after 4h of irradiation, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 4 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 60%, and the selectivity is more than 99%.
Example 5, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 0.5mmol of pentahydrate bismuth nitrate and 1mmol of sodium oleate into 10mL of water, stirring at the speed of 800r/m for 0.5h, then adding 0.25mmol of sodium molybdate, stirring at the speed of 800r/m for 1h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 170 ℃ for 12h, centrifuging, collecting precipitate, centrifuging and washing with water and absolute ethyl alcohol for three times respectively, drying at 60 ℃ for 15h, and obtaining Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 20mg of quantum dots in 2mL of water, adding 10.4 microliters of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at the speed of 800r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after 2h of irradiation, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 2 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 30%, and the selectivity is more than 99%.
Example 6, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
0.5mmol bismuth nitrate pentahydrate and 3mmol sodium oleate are added to 40mL water, stirred at 700r/m for 1h, then 0.25mmol sodium molybdate is added, stirred well at 700r/m for 2h, and then transferred to 100mL in a high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 18h at 160 ℃, centrifugally collecting precipitates, centrifugally washing the precipitates with water and absolute ethyl alcohol for three times respectively, and drying the precipitates for 17h at 60 ℃ to obtain Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 15mg of quantum dots in 1.5mL of water, adding 10.4 microliters of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at the speed of 600r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after the light is irradiated for 8 hours, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 8 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 58%, and the selectivity is more than 99%.
Example 7, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 1mmol of pentahydrate bismuth nitrate and 2mmol of sodium oleate into 50mL of water, stirring at the speed of 1000r/m for 1h, then adding 0.5mmol of sodium molybdate, fully stirring at the speed of 1000r/m for 1h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 170 ℃ for 20h, centrifuging, collecting precipitate, respectively carrying out centrifugal washing with water and absolute ethyl alcohol for three times, and drying at 60 ℃ for 12h to obtain Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 15mg of quantum dots in 1mL of water, adding 10.4 microliters of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at the speed of 800r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after the light source is irradiated for 3 hours, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 3h under visible lightThe conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 43 percent, and the selectivity is more than 99 percent.
Example 8, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 1mmol of pentahydrate bismuth nitrate and 3mmol of sodium oleate into 30mL of water, stirring at the speed of 900r/m for 0.5h, then adding 0.5mmol of sodium molybdate, stirring fully at the speed of 900r/m for 2h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 190 ℃ for 12h, centrifuging, collecting precipitate, respectively carrying out centrifugal washing with water and absolute ethyl alcohol for three times, drying at 60 ℃ for 22h, and obtaining Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 15mg of quantum dots in 1.5mL of water, adding 20.8 microliter of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at 900r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after 5h of irradiation, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 5 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 44%, and the selectivity is more than 99%.
Example 9, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 1mmol bismuth nitrate pentahydrate and 4mmol sodium oleate into 60mL water, stirring at 850r/m for 1h, adding 0.5mmol sodium molybdate, stirring at 850r/m for 1h, transferring to 100mL high-pressure reaction kettle with polytetrafluoroethylene lining, performing hydrothermal reaction at 200 ℃ for 10h, centrifuging to collect precipitate, respectively washing with water and anhydrous ethanol for three times, and drying at 60 ℃ for 14h to obtain Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Quantum dot 15mg, dispersed in 1.5mL water, added 20.8. mu.L benzylIntroducing oxygen into alcohol, discharging air in the reaction flask, sealing, stirring at 600r/m for 30m, starting 500W xenon lamp for irradiation, filtering ultraviolet light below 420nm from the light source with optical filter, finishing reaction after 5h of illumination, centrifuging to filter Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 5 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 52%, and the selectivity is more than 99%.
Example 10, Bi in this example2MoO6The preparation method of the quantum dot is carried out according to the following steps:
adding 1mmol of pentahydrate bismuth nitrate and 6mmol of sodium oleate into 80mL of water, stirring at 850r/m for 1h, adding 0.5mmol of sodium molybdate, stirring at 850r/m for 1.5h, transferring to 100mL of a high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 180 ℃ for 15h, centrifuging, collecting precipitate, respectively carrying out centrifugal washing with water and absolute ethyl alcohol for three times, and drying at 60 ℃ for 24h to obtain Bi2MoO6And (4) quantum dots.
Bi prepared in this example was taken2MoO6Dispersing 20mg of quantum dots in 2mL of water, adding 10.4 microliters of benzyl alcohol, introducing oxygen to discharge air in a reaction bottle, sealing, stirring at 850r/m for 30m, starting a 300W xenon lamp for irradiation, filtering ultraviolet light below 420nm in a light source by using an optical filter, finishing the reaction after 4h of irradiation, and centrifugally filtering Bi2MoO6And (3) quantum dots, wherein the content of benzyl alcohol and benzaldehyde in the solution is detected by using a gas chromatograph-mass spectrometer. Upon detection, Bi prepared in this example2MoO6The quantum dots are irradiated for 4 hours under visible light, the conversion rate of the benzyl alcohol oxidized into the benzaldehyde is 52%, and the selectivity is more than 99%.
Claims (10)
1. Bi2MoO6Quantum dot, characterized in that said Bi2MoO6The quantum dots take pentahydrate bismuth nitrate and sodium molybdate as raw materials, take sodium oleate as a surfactant, and adopt a hydrothermal methodIs prepared by the following steps.
2. The Bi according to claim 12MoO6The quantum dot is characterized in that the molar ratio of bismuth nitrate pentahydrate to sodium molybdate is 2: 1.
3. The Bi of claim 22MoO6The quantum dot is characterized in that the molar ratio of the bismuth nitrate pentahydrate to the sodium oleate is 1: 2-6.
4. A Bi of claim 1, 2 or 32MoO6The preparation method of the quantum dot is characterized by comprising the following steps:
dispersing pentahydrate bismuth nitrate and sodium oleate in water, and stirring for 0.5-1 h. Then adding sodium molybdate, and continuing stirring for 1-2 h;
step two, carrying out hydrothermal reaction, after the reaction is finished, centrifugally separating and collecting precipitates, respectively centrifugally washing the precipitates for at least 3 times by using water and absolute ethyl alcohol, and drying the precipitates to obtain Bi2MoO6And (4) quantum dots.
5. The Bi according to claim 42MoO6The preparation method of the quantum dot is characterized in that the volume ratio of the mole of the bismuth nitrate pentahydrate to the volume of the water in the step one is 1mmol to (20-80) mL.
6. The Bi according to claim 42MoO6The preparation method of the quantum dot is characterized in that stirring is carried out at the speed of 500r/m-1000r/m in the step one.
7. The Bi according to claim 42MoO6The preparation method of the quantum dot is characterized in that the reaction is carried out for 10 to 24 hours at the temperature of 160 to 200 ℃ in the second step.
8. The Bi according to claim 42MoO6The preparation method of the quantum dot is characterized in thatAnd reacting at 180 ℃ for 20h in the second step.
9. The Bi according to claim 42MoO6The preparation method of the quantum dot is characterized in that the step two is dried for 12 to 24 hours at the temperature of between 60 and 80 ℃.
10. A Bi of claim 1, 2 or 32MoO6Quantum dots are used as photocatalysts.
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| CN112777637A (en) * | 2020-12-23 | 2021-05-11 | 浙江工业大学 | High-activity defective Bi2MoO6Nanobelt and preparation and application thereof |
| CN113275003A (en) * | 2021-05-17 | 2021-08-20 | 南昌航空大学 | Molybdenum dioxide/bismuth photocatalyst and preparation method and application thereof |
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| CN109569580A (en) * | 2018-11-29 | 2019-04-05 | 南昌航空大学 | A kind of composite photocatalyst and its preparation method and application |
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| CN107349926A (en) * | 2017-07-18 | 2017-11-17 | 福州大学 | Monolayer bismuth molybdate nanometer sheet and its application in photochemical catalytic oxidation benzylalcohol to aldehyde |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112777637A (en) * | 2020-12-23 | 2021-05-11 | 浙江工业大学 | High-activity defective Bi2MoO6Nanobelt and preparation and application thereof |
| CN112777637B (en) * | 2020-12-23 | 2022-07-08 | 浙江工业大学 | High-activity defective Bi2MoO6Nano belt and preparation and application thereof |
| CN113275003A (en) * | 2021-05-17 | 2021-08-20 | 南昌航空大学 | Molybdenum dioxide/bismuth photocatalyst and preparation method and application thereof |
| CN113275003B (en) * | 2021-05-17 | 2023-01-06 | 南昌航空大学 | Molybdenum dioxide/bismuth photocatalyst and preparation method and application thereof |
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Application publication date: 20200317 |